Reddish-brown sulfur dye.



urrs s'r'rs PATENT- FFIGEI FRITZ LEHMANN; OF VOHWINKEL,

NEAR ELBERFELD, GhRMAuY, Assiouos T FARBEN- FABRIKEN VOltll lL FRlEDR. BAYER e00 OF EIIBERFELD, GERMANY, A CORPORATION OF GEItMANYr .15 peei flcation of Letters Patent.

REDDISH- BROWN SULFUR Patented Sept. .24, 1907.

Application filed July. 22, 1907-' Serial No. 385 053l To all whom it may concern: I

Be it known that I, Farrz LEHMANN, doctor of philosophy chemist, a citizen of, the German Empire, residing at Vohwinkel, near Elberfeld, Germany, have invented new and useful Improvements in Reddish- 1 Brown Sulfur Dyes, of 'which the following is a specificationj V In the specification for Letters Patent No. 818,980 dated April 1906 there is described the preparation of a sulfin dye by heating with alkali polysulfid in th'e'pre'sen cle. of "substances containing nopper the aminooxytoliiph'enaz in of the following formula:

Lil/

' This compound see Example no: the said-specificaalkaline sulfid' melt without the addition of copper compounds, and (2) becailse thedyeings of the colors. prepared without the addition of copper compounds by a subsequent treatment with copper on, fiber become muddy blue.

I have now-found that aminooxytoluphenazin' when heated under certain conditions with alkalipolysulfid without the addition of copper or copper compounds directly yields a valuable clear reddish-brown dye,

which of course is free from copper and the dyeings of which on subsequent treatment with copper are.not

changed into muddy-bluebut remain brown. My dye is, therefore, not anticipated by the specification of the said Letters Patent 818,980, inasmuchas the dye described there as obtainable from aminooxytoluphenazin exhibits properties entirely different from.

those 'offthe dye which forms the object of my present invention. I

The following eiiample will serve to further illus trate the nature of my invention and the method of carrying it into practical effect, the parts being by weight: 15,8 parts of paraaminophenol and 18 parts of metatoluylen'diamin are dissolved in 1000 parts of cold water. 10 parts of ammonia (20%) and parts of manganperoxid are subsequently added. The

Ex'argple I of the same specification). It has been mixture is as fast as possible heatedtozboiling and energetically boiled for about twohours. 50 parts of soda-lye containing 27 percent'of NaOH are added,

the liquid is filtered and thehy'drochlorid of the aminooxytoluphenazin is precipitated from the filtrate LY by the addition of common salt and an excess of hydrochloric acid. The resulting precipitate is pressed and subsequently mixed with .such a quantity of a say 20 pe'r cental sodiumsulfid solution as corresponds with 42 parts of pure Na s, and with 80 parts of sulfur; The mixture is heated with evaporation of water, until'the temperature of the heated mass is 135 centigrade. At this temperature tile mass is kept for about 7 20 hours employing a reflux condenser. After this;

time the melt is' dried and subsequently ground.

The color is thus obtained in the form of a dark brown powder. It can be used directly'for dyeing. I

My new dyestuff shows the following reactions: It

is very easily soluble water in the presence of sodium sulfid with a blackish-brown color, itis practically insoluble in soda-lye containing 27-;per cent of 'NaOH,- it dissolves in concentrated sulfuric. acid (66 Baum) with a dark brown color which by the addition of water first becomes redder a dark reddish-brown precipitate 'being fina1ly separated. It dyes unmordantedcotton in a bath of sodium sulfid reddish-brown shades of great fastness the dyeings thus obtained remaining brown when treated on the fiber with copper salts.

Having thus described my invention and in what manner the same is to be performed, what I claim as I new, and desire to secure by Letters Patent, is:

The horeln-described new reddish-brown sulfur dye obtalnable by meltlng amluoonytoluphenazln of thetorniula with alkaline sulfld and sulfur at about 185 centigrade, beluga dark: brown powder very easlly soluble in water In the presence of sodlum sulfidwlth a blackish brown color, belng practically insoluble in soda-lye conta'lnlng 27 per cent of NaOH, belng dissolved by concentrated sulturleacld (86 Be) with a dark brown color whlch by the addltlonof water first becomes redder, a

dark reddish-brown lnsolublepreclpltate being finally,

separated, dyelng unmordanted i'bttou In a bath of sodlum sulfid reddish-brown shades ,of great fastuess,-the dyelngs thus obtalned remalnlng brown when treated on the;

fiber with copper salts,. substantially as herelnhefore descrlbell.

In testlmony whereof I have hereunto set my hand in the presence of two subscribing witnesses.

FRITZLEHMANN. [L. 5.1

Witnesses:

O'r'ro-Kmns, QSKAB KLuo. j- 

